CN114644520A - Pink nano zirconia ceramic and preparation method thereof - Google Patents
Pink nano zirconia ceramic and preparation method thereof Download PDFInfo
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- CN114644520A CN114644520A CN202210430286.1A CN202210430286A CN114644520A CN 114644520 A CN114644520 A CN 114644520A CN 202210430286 A CN202210430286 A CN 202210430286A CN 114644520 A CN114644520 A CN 114644520A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 239000000919 ceramic Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 46
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011268 mixed slurry Substances 0.000 claims abstract description 22
- 150000003746 yttrium Chemical class 0.000 claims abstract description 22
- 150000003754 zirconium Chemical class 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 12
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 23
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 22
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 18
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical group O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 7
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229910001940 europium oxide Inorganic materials 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 11
- 238000004040 coloring Methods 0.000 description 10
- 239000003086 colorant Substances 0.000 description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010295 mobile communication Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention relates to pink nano zirconia ceramic and a preparation method thereof, wherein the pink nano zirconia ceramic comprises 80-100 parts of soluble zirconium salt, 3-10 parts of soluble yttrium salt, 0.1-5 parts of titanium dioxide and 0.01-2 parts of metal oxide by weight. The preparation method comprises the following steps: dissolving soluble zirconium salt, soluble yttrium salt, titanium dioxide and metal oxide in water to obtain a mixed solution; carrying out hydrothermal reaction to obtain mixed slurry; adjusting the pH value of the mixed slurry to be alkaline, and then cleaning, spray drying and calcining to obtain pink nano zirconia ceramic powder; grinding zirconia ceramic powder, adding an additive, uniformly mixing, granulating, dry-pressing and molding the granulated powder, and sintering a green blank to obtain the pink nano zirconia ceramic. The ceramic material prepared by the preparation method has the advantages of beautiful and excellent pink color, good color development, stable color generation and effective guarantee of the strength performance of the ceramic material.
Description
Technical Field
The invention relates to pink nanometer zirconia ceramic and a preparation method thereof, belonging to the technical field of ceramic materials.
Background
The zirconia ceramic is a novel high-technology ceramic with low shielding, high strength, wear resistance, high temperature resistance and corrosion resistance. The optical fiber connector component has good communication performance and can be used for producing optical fiber connector components for communication; the strength is high, the Mohs hardness is about 8.5, and the hardness is similar to that of sapphire, so that the artificial tooth can be used for manufacturing artificial teeth, cutting tools, golf club heads, simulated gems and the like; the chemical stability is also good, and the method is widely applied to the field of high-temperature insulation and sealing devices; in addition, the method has sensitive characteristics and can be used for producing fuel cell membranes, oxygen sensors and the like. Compared with metal, the zirconia ceramic can better meet the requirement of 5G communication; compared with glass, the ceramic is more attractive and delicate, and is resistant to falling and wear.
Zirconia materials are preferred materials for the outer housing components of mobile communication devices due to their good overall performance. The exterior housing parts of mobile communication devices currently on the market are single in color and cannot meet the needs of the public.
At present, two main methods for coloring zirconia ceramics are available, one is an external coloring method by using a coloring liquid, namely, soaking and external coloring are carried out on a pre-sintered zirconia blank. The dyeing method adopting the dyeing liquid is simple to operate, but is easy to color unevenly and is greatly influenced by operation; the other method is an internal coloring method, and a colorant is added in the preparation process of the zirconia powder, so that the zirconia ceramic can be uniformly and stably colored. However, after the internal coloring method is doped with the colorant, the internal coloring method has certain influence on properties such as the crystal phase and the density of the material, and partial metal oxides have large influence on the mechanical property and the translucency of the zirconia material, so that the use requirement cannot be met. In addition, the sintering temperature of the zirconia ceramic is relatively high, generally 1400-1700 ℃, and at the temperature, most coloring agents can be reduced in color and even can not be reduced to the color any more.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides pink nano zirconia ceramic and a preparation method thereof.
The technical scheme for solving the technical problems is as follows: the pink nano zirconia ceramic comprises, by weight, 80-100 parts of soluble zirconium salt, 3-10 parts of soluble yttrium salt, 0.1-5 parts of titanium dioxide and 0.01-2 parts of metal oxide.
Further, the soluble zirconium salt is zirconium oxychloride octahydrate; the soluble yttrium salt is one or a combination of yttrium chloride, yttrium nitrate and yttrium acetate.
Further, the metal oxide is iron oxide and rare earth metal oxide, and the rare earth metal oxide is one or any two of erbium oxide, europium oxide and holmium oxide.
The invention also discloses a preparation method of the pink nano zirconia ceramic, which comprises the following steps:
s1, dissolving soluble zirconium salt, soluble yttrium salt, titanium dioxide and metal oxide in water to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution to obtain mixed slurry;
s3, adjusting the pH of the mixed slurry to be alkaline, and then cleaning, spray drying and calcining to obtain pink nano zirconia ceramic powder;
and S4, grinding the pink nano zirconia ceramic powder obtained in the step S3, adding an additive, uniformly mixing, granulating, dry-pressing and molding the granulated powder, and sintering a green blank to obtain the pink nano zirconia ceramic.
Further, the specific process of step S1 is: adding soluble zirconium salt into water to prepare 80-100 wt% of zirconium salt aqueous solution, then adding soluble yttrium salt into water to prepare 3-10 wt% of yttrium salt aqueous solution, mixing the zirconium salt aqueous solution and the yttrium salt aqueous solution, adding titanium dioxide and metal oxide, and heating and dissolving at the dissolving temperature of 60-90 ℃.
Further, in step S2, the hydrothermal reaction temperature is 80-200 ℃ and the hydrothermal reaction time is 10-120 h.
Further, in step S3, the specific operation of adjusting the pH of the mixed slurry to alkaline is: and dropwise adding ammonia water into the mixed slurry while stirring, and adjusting the pH of the mixed slurry to 8-12, wherein the concentration of the ammonia water is 4% -20%.
Further, in step S3, the mixed slurry adjusted to be alkaline is circularly cleaned in a ceramic filter machine, and is spray-dried after being cleaned; the calcining temperature is 600-1100 ℃, and the calcining time is 1-10h, so that pink nano zirconia ceramic powder is obtained.
Further, in step S4, the pink nano zirconia ceramic powder obtained in step S3 is ground, the solid content in the grinding process is 20% to 60% (that is, water needs to be added in the grinding process to obtain slurry, the mass ratio of the solid in the slurry is the solid content), the ground powder is granulated to obtain granulated powder, the average particle size of the granulated powder is 30 nm to 50nm, the addition amount of the additive is 1% to 5% of the mass of the mixed solution obtained in step S1, and the dispersant is one or a combination of polyethylene glycol, ammonium polyacrylate and acrylic resin.
Further, in step S4, the sintering temperature of the green compact is 1300-1400 ℃, and the sintering time is 1-10 h.
The invention has the beneficial effects that:
(1) the invention selects proper metal oxide as colorant, has unique optical property, good luminescence property and stable color generation, selects erbium oxide, europium oxide and holmium oxide, can obtain pink zirconia ceramic with excellent aesthetic feeling, and can be applied to the external shell part of mobile communication equipment;
(2) the zirconia ceramic material of the invention can properly reduce the sintering temperature and reduce the grading and volatilization of the colorant by doping a proper amount of titanium dioxide, thereby ensuring that the coloring effect of the colorant is more excellent;
(3) the zirconia ceramic material has the advantages of easy sintering in the preparation process, stable and uniform color, simple preparation method process, easy operation and stable product performance, and the density of the final pink nano zirconia ceramic sintered body can reach 6.05-6.09g/cm3The bending strength can reach 1150-1200 MPa.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
The pink nanometer zirconia ceramic comprises, by weight, 93 parts of zirconium oxychloride octahydrate, 5.2 parts of yttrium chloride, 1 part of titanium dioxide, 0.2 part of ferric oxide, 0.3 part of erbium oxide and 0.3 part of europium oxide.
The preparation method comprises the following steps:
s1, dissolving zirconium oxychloride octahydrate in water to prepare 93 wt% of zirconium salt aqueous solution; dissolving yttrium chloride in water to prepare 5.2 wt% yttrium salt water solution; after mixing the zirconium salt aqueous solution and the yttrium salt aqueous solution, adding titanium dioxide, iron oxide, erbium oxide and europium oxide, and heating for dissolving at the dissolving temperature of 85 ℃ to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution at 200 ℃ for 96h to obtain mixed slurry;
s3, dropwise adding 25% ammonia water into the mixed slurry, stirring while dropwise adding, and adjusting the final pH value of the slurry to 10; cleaning the zirconium oxide powder by using a filter membrane machine until the conductivity is less than 500us/cm, drying the zirconium oxide powder in a spray dryer, and calcining the zirconium oxide powder for 3 hours at the temperature of 1000 ℃ to obtain pink nano zirconium oxide powder;
s4, grinding the nano zirconia powder obtained in the step S3, wherein the solid content in the grinding process is 30%, adding polyethylene glycol accounting for 3% of the mass of the mixed solution after grinding as an additive, uniformly mixing, granulating to obtain granulated powder with the particle size of 30-50nm, carrying out dry pressing on the granulated powder, and sintering the green body at 1400 ℃ for 4 hours to obtain a pink nano zirconia ceramic pre-sintered body.
The density of the pink nano zirconia ceramic pre-sintered body ceramic block obtained in the embodiment is 6.08g/cm3Is pink, has uniform and stable color, and the specific surface area of the pink nano zirconia powder for manufacturing the pink nano zirconia ceramic pre-sintered body is 3-25m2The pre-sintered body was tested to have a flexural strength of 1175MPa and a hardness of 11.7 GPa.
Example 2
The pink nano zirconia ceramic comprises, by weight, 92 parts of zirconium oxychloride octahydrate, 6.3 parts of yttrium chloride, 1.1 parts of titanium dioxide, 0.3 part of iron oxide and 0.3 part of holmium oxide.
The preparation method comprises the following steps:
s1, dissolving zirconium oxychloride octahydrate in water to prepare a 92 wt% zirconium salt aqueous solution; dissolving yttrium chloride in water to prepare a 6.3 wt% yttrium salt aqueous solution; after mixing the zirconium salt aqueous solution and the yttrium salt aqueous solution, adding titanium dioxide, iron oxide and holmium oxide, and heating for dissolving at the dissolving temperature of 85 ℃ to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution at 180 ℃ for 120h to obtain mixed slurry;
s3, dropwise adding 20% ammonia water into the mixed slurry while stirring, and adjusting the final pH value of the slurry to 11; cleaning by using a filter membrane machine, spray drying, and calcining for 5 hours at 850 ℃ to obtain pink nano zirconium oxide powder;
s4, grinding the nano zirconia powder obtained in the step S3, wherein the solid content in the grinding process is 60%, adding ammonium polyacrylate accounting for 5% of the mass of the mixed solution after grinding, uniformly mixing, granulating to obtain granulated powder with the particle size of 30-50nm, carrying out dry pressing on the granulated powder, and sintering the green blank at 1350 ℃ for 5 hours to obtain a pink nano zirconia ceramic pre-sintered body.
The density of the pink nano zirconia ceramic pre-sintered body ceramic block obtained in the embodiment is 6.09g/cm3Is pink, has uniform and stable color, and the specific surface area of the pink nano zirconia powder for manufacturing the pink nano zirconia ceramic pre-sintered body is 3-25m2The pre-sintered body was tested to have a flexural strength of 1200MPa and a hardness of 12.2 GPa.
Example 3
The pink nano zirconia ceramic comprises, by weight, 80 parts of zirconium oxychloride octahydrate, 3.0 parts of yttrium nitrate, 0.1 part of titanium dioxide, 0.1 part of ferric oxide and 0.1 part of erbium oxide.
The preparation method comprises the following steps:
s1, dissolving zirconium oxychloride octahydrate in water to prepare 80 wt% of zirconium salt aqueous solution; dissolving yttrium chloride in water to prepare a 3.0 wt% yttrium salt aqueous solution; mixing a zirconium salt aqueous solution and an yttrium salt aqueous solution, adding titanium dioxide, iron oxide and erbium oxide, and heating to dissolve at the dissolving temperature of 60 ℃ to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution at 100 ℃ for 20 hours to obtain mixed slurry;
s3, dropwise adding 15% ammonia water into the mixed slurry while stirring, and adjusting the final pH value of the slurry to 8; and (3) cleaning by using a filter membrane machine, spray-drying, and calcining for 2h at 600 ℃ to obtain pink nano zirconium oxide powder.
S4, grinding the nano zirconia powder obtained in the step S3, wherein the solid content in the grinding process is 45%, adding acrylic resin accounting for 1% of the mass of the mixed solution after grinding, uniformly mixing, granulating to obtain granulated powder with the particle size of 30-50nm, carrying out dry pressing on the granulated powder, and sintering the green blank at 1300 ℃ for 2 hours to obtain a pink nano zirconia ceramic pre-sintered body.
The density of the pink nano zirconia ceramic pre-sintered body ceramic block obtained in the embodiment is 6.06g/cm3Is pink, has uniform and stable color, and the specific surface area of the pink nano zirconia powder for manufacturing the pink nano zirconia ceramic pre-sintered body is 3-25m2The pre-sintered body was tested for 1170Mpa bending strength and 11.9GPa hardness.
Example 4
The pink nano zirconia ceramic comprises, by weight, 100 parts of zirconium oxychloride octahydrate, 10.0 parts of yttrium acetate, 5 parts of titanium dioxide, 0.3 part of iron oxide, 0.3 part of erbium oxide and 0.4 part of holmium oxide.
The preparation method comprises the following steps:
s1, dissolving zirconium oxychloride octahydrate in water to prepare a 100 wt% zirconium salt aqueous solution; dissolving yttrium chloride in water to prepare a 10.0 wt% yttrium salt aqueous solution; after mixing the zirconium salt aqueous solution and the yttrium salt aqueous solution, adding titanium dioxide, iron oxide, erbium oxide and holmium oxide, and heating for dissolving at the dissolving temperature of 90 ℃ to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution at 200 ℃ for 100h to obtain mixed slurry;
s3, dropwise adding 4% ammonia water into the mixed slurry while stirring, and adjusting the final pH value of the slurry to 12; and (3) cleaning by using a filter membrane machine, spray-drying, and calcining for 9 hours at 1100 ℃ to obtain pink nano zirconium oxide powder.
S4, grinding the nano zirconia powder obtained in the step S3, wherein the solid content in the grinding process is 40%, adding ammonium polyacrylate accounting for 3% of the mass of the mixed solution after grinding, uniformly mixing, granulating to obtain granulated powder with the particle size of 30-50nm, carrying out dry pressing on the granulated powder, and sintering the green blank at 1400 ℃ for 6 hours to obtain a pink nano zirconia ceramic pre-sintered body.
The density of the pink nano zirconia ceramic pre-sintered body ceramic block obtained in the embodiment is 6.08g/cm3Is pink, has uniform and stable color, and the specific surface area of the pink nano zirconia powder for manufacturing the pink nano zirconia ceramic pre-sintered body is 3-25m2The pre-sintered body was tested to have a flexural strength of 1185MPa and a hardness of 11.5 GPa.
Comparative example 1
The pink nano zirconia ceramic was prepared by the same method as in example 2 except that titanium dioxide was not added and the sintering temperature in step S4 was 1600 ℃.
The density of the pink nano zirconia ceramic pre-sintered body ceramic block obtained by the comparative example is 6.09g/cm3It was pink and uniform in color, but the color was relatively lighter than that of the pink nano-zirconia ceramic of example 2, and the specific surface area of the pink nano-zirconia powder for producing the pre-sintered body of the pink nano-zirconia ceramic was 3 to 25m2The pre-sintered body was tested for a flexural strength of 1032MPa and a hardness of 10.2 GPa.
From the comparison of example 2 and comparative example 1, it can be seen that: the addition of titanium dioxide can effectively reduce the sintering temperature, thereby improving the coloring effect and avoiding the decomposition and volatilization of the colorant.
Comparative example 2
The nano zirconia ceramic was prepared by the same method as in example 2 except that the calcination temperature in step S3 was 1500 ℃.
The density of the nano zirconia ceramic pre-sintered body ceramic block obtained by the comparative example is 6.02g/cm3The specific surface area of the nano zirconia powder for manufacturing the nano zirconia ceramic pre-sintered body is 3 to 25m2The pre-sintered body was tested for a flexural strength of 1013MPa and a hardness of 10.6 GPa.
From the comparison of example 2 and comparative example 2, it can be seen that: too high a calcination temperature may affect the coloring effect.
Comparative example 3
The nano zirconia ceramics were prepared by the same method as in example 3 except that iron oxide was not added.
The density of the nano zirconia ceramic pre-sintered body ceramic block obtained by the comparative example is 6.04g/cm3The specific surface area of the nano zirconia powder for preparing the nano zirconia ceramic pre-sintered body is 3 to 25m2The pre-sintered body was tested for a flexural strength of 1195MPa and a hardness of 12.0 GPa.
From the comparison of example 2 and comparative example 3, it can be seen that: the pink nano zirconia ceramics with excellent aesthetic feeling can be obtained only by using the iron oxide and the rare earth metal oxide together.
Comparative example 4
The nano zirconia ceramics were prepared by the same method as in example 1 except that the drying was directly performed without spray drying. Calcining at 1000 ℃, and grinding to obtain pink nano zirconia powder with the particle size of 150-200 nm;
the density of the ceramic block of the pre-sintered body of pink nano zirconia ceramic obtained in the embodiment is 5.93g/cm3Compared with example 1, the zirconia ceramic has density and strength which can not meet the requirements, and it can be seen that: the mode of spray drying is reducedThe particle size of the powder is low, the agglomeration is reduced, and the quality of the ceramic is improved.
Comparative example 5
The nano zirconia ceramic was prepared by the same method as in example 4 except that the grinding solid content was 19%. The particle size of the obtained pink nano zirconia powder is 100-150 nm;
the density of the ceramic block of the pre-sintered body of pink nano zirconia ceramic obtained in the embodiment is 6.02g/cm3The choice of the milled solids content will affect the powder particle size compared to example 4, resulting in a reduced bulk density.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The pink nano zirconia ceramic is characterized by comprising, by weight, 80-100 parts of soluble zirconium salt, 3-10 parts of soluble yttrium salt, 0.1-5 parts of titanium dioxide and 0.01-2 parts of metal oxide.
2. The pink nano zirconia ceramic according to claim 1, wherein the soluble zirconium salt is zirconium oxychloride octahydrate; the soluble yttrium salt is one or a combination of yttrium chloride, yttrium nitrate and yttrium acetate.
3. The pink nano zirconia ceramic according to claim 1, wherein the metal oxide is iron oxide and rare earth metal oxide, and the rare earth metal oxide is one or a mixture of any two of erbium oxide, europium oxide and holmium oxide.
4. A method for preparing the pink nano zirconia ceramic according to any one of claims 1 to 3, which comprises the following steps:
s1, dissolving soluble zirconium salt, soluble yttrium salt, titanium dioxide and metal oxide in water to obtain a mixed solution;
s2, carrying out hydrothermal reaction on the mixed solution to obtain mixed slurry;
s3, adjusting the pH of the mixed slurry to be alkaline, then cleaning until the conductivity is less than 500us/cm, spray drying, and calcining to obtain pink nano zirconia ceramic powder;
and S4, grinding the pink nano zirconia ceramic powder obtained in the step S3, adding an additive, uniformly mixing, granulating, dry-pressing and molding the granulated powder, and sintering a green blank to obtain the pink nano zirconia ceramic.
5. The method for preparing pink nano zirconia ceramic according to claim 4, wherein the specific process of step S1 is as follows: adding soluble zirconium salt into water to prepare 80-100 wt% of zirconium salt aqueous solution, then adding soluble yttrium salt into water to prepare 3-10 wt% of yttrium salt aqueous solution, mixing the zirconium salt aqueous solution and the yttrium salt aqueous solution, adding titanium dioxide and metal oxide, and heating and dissolving at the dissolving temperature of 60-120 ℃.
6. The method for preparing pink nano zirconia ceramic according to claim 4, wherein in step S2, the hydrothermal reaction temperature is 80-200 ℃ and the hydrothermal reaction time is 10-120 h.
7. The method for preparing pink nano zirconia ceramic according to claim 4, wherein the specific operation of adjusting the pH of the mixed slurry to be alkaline in step S3 is as follows: and dropwise adding ammonia water into the mixed slurry while stirring, and adjusting the pH of the mixed slurry to 8-12, wherein the concentration of the ammonia water is 4% -20%.
8. The method for preparing pink nano zirconia ceramic according to claim 4, wherein in step S3, the mixed slurry adjusted to be alkaline is circularly cleaned in a ceramic membrane filter, and is spray-dried after being cleaned; the calcination temperature is 600-1100 ℃, and the calcination time is 1-10 h.
9. The method for preparing pink nano zirconia ceramic according to claim 4, wherein in step S4, in step S4, the solid content in the grinding process is 20% to 60%, and the average particle size of the granulated powder is 30 to 50 nm; the additive is added in an amount of 1-5% of the mass of the mixed solution prepared in the step S1, and the additive is one or a combination of polyethylene glycol, ammonium polyacrylate and acrylic resin.
10. The method as claimed in claim 4, wherein in step S4, the green body sintering temperature is 1300-1400 ℃, and the sintering time is 1-10 h.
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